title: Optimized determination of polybrominated diphenyl ethers and polychlorinated biphenyls in sheep serum by solid-phase extraction-gas chromatography-mass spectrometry.
abstract: We describe a solid-phase extraction (SPE) method, followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous determination of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in sheep serum samples. The denaturation of serum proteins by formic acid, water-1-propanol and water-2-propanol were compared and optimized. Seven different solid-phase sorbents were tested and it was found that Strata-X cartridge (200mg, 6 mL) gave the best recoveries (92-106%, SD<6%, n=3) for all the target analytes. The different extraction solvents (iso-hexane and dichloromethane), either alone or in combination, were used to extract these persistent organic compounds from spiked serum samples by SPE. Removal of co-extracted biogenic materials was achieved using adsorption chromatography with acid modified silica and activated silica. Iso-hexane was found to be the most appropriate solvent for clean-up providing good recoveries and clear chromatographic separation; its use is preferable to that of DCM because it is less environmentally toxic. The limits of detection (LOD) of the proposed method were 47-105 pg g(-1) and 16-24 pg g(-1) for the different PBDEs and PCBs studied, respectively. The developed method was linear over the range from 0.05 to 30 ng g(-1), for all PBDEs except PBDE 183 (0.10-30 ng g(-1)), and from 0.02 to 30 ng g(-1) for all tested PCB congeners. The established method was successfully applied to sheep serum samples from Scotland, UK, for the determination of the target PBDEs and PCBs.
authors.affiliation: The Macaulay Land Use Research Institute, Analytical Group, Craigiebuckler, Aberdeen AB15 8QH, UK. z.zhang@macaulay.ac.uk
authors.forename: Zulin
authors.initials: Z
authors.lastname: Zhang
authors.forename: Stewart M
authors.initials: SM
authors.lastname: Rhind
mesh_terms: D000818:Animals; D001798:Blood Proteins / Q000378:metabolism; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D055768:Halogenated Diphenyl Ethers / Q000097:blood*; D057230:Limit of Detection; D011078:Polychlorinated Biphenyls / Q000097:blood*; D012756:Sheep; D052616:Solid Phase Extraction / Q000379:methods*
chemical_list: D001798:Blood Proteins; D055768:Halogenated Diphenyl Ethers; D011078:Polychlorinated Biphenyls